ASTM_D_5910_-_05_2012.pdf

Designation:D591005(Reapproved 2012)Standard Test Method forDetermination of Free Formaldehyde in Emulsion Polymersby Liquid Chromatography1This standard is issued under the fixed designation D5910;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method is used for the determination of freeformaldehyde(HCHO)in emulsion polymers without upset-ting existing formaldehyde equilibria.The procedure has beenevaluated using acrylic,acrylonitrile-butadiene,carboxylatedstyrene-butadiene and polyvinyl acetate emulsion polymers.This test method may also be applicable for emulsion polymersof other compositions.The established working range of thistest method is from 0.05 to 15 ppm formaldehyde.Emulsionpolymers must be diluted to meet the working range.1.2 This test method minimizes changes in free formalde-hyde concentration that can result from changes in the physicalor chemical properties of an emulsion polymer.1.3 There are no known limitations to this test method whenused in the manner described.The emulsion polymer testspecimen must be prepared with a diluent that has a pH similarto that of the emulsion.Use of an inappropriate pH may upsetformaldehyde equilibria and result in incorrect formaldehydelevels.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD2194 Test Method for Concentration of FormaldehydeSolutionsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E682 Practice for Liquid Chromatography Terms and Rela-tionships3.Summary of Test Method3.1 The aqueous phase of an emulsion polymer is dilutedand chromatographed on a reversed-phase octadecyl silane(ODS)column using an aqueous mobile phase and a visible-light detector at 410 nm.Formaldehyde is separated from otherspecies in the matrix on a chromatographic column.Thedetection system includes a post-column reactor that producesa lutidine derivative when formaldehyde reacts with the2,4-pentanedione reagent(Nash Reagent).The concentrationof free formaldehyde in emulsion polymers is determined usingpeak areas from the standard and sample chromatograms.Thistest method is specific for formaldehyde.4.Significance and Use4.1 With the need to calculate free formaldehyde levels inemulsion polymers,it is necessary to make the determinationwithout upsetting any equilibria that might generate or depleteformaldehyde.This test method provides a means for deter-mining ppm levels of free formaldehyde in emulsion polymerswithout upsetting existing equilibria.5.Interferences5.1 This test method is very selective for formaldehyde.Potential interferants are either chromatographically separatedfrom formaldehyde or do not react with the post-columnreagent.NOTE1The following species were identified as possible interfer-ences for the method:acetaldehyde,acetone,benzaldehyde,formamide,formic acid,glyoxylic acid and propionaldehyde.These species,whenchromatographed using this test method,did not interfere with theformaldehyde peak at the 1000 ppm level or lower.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.33 on Polymers and Resins.Current edition approved Nov.1,2012.Published November 2012.Originallyapproved in 1996.Last previous edition approved in 2005 as D5910 05.DOI:10.1520/D5910-05R12.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.2 Because emulsion polymers vary in composition,themethod run time may need to be extended to allow for lateeluting compounds.Compounds that remain on the columnafter an analysis may interfere with the formaldehyde peak insubsequent runs.6.Apparatus6.1 Liquid ChromatographAny liquid chromatographicinstrument having an injection valve,a post-column reactor,a410-nm UV-Vis detector,and an isocratic solvent deliverysystem may be used.The solvent delivery system must delivera mobile